固相微萃取-便携式气相色谱-串联质谱法现场测定水中的2-甲基异莰醇和土臭素
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摘要
建立了固相微萃取-便携式气相色谱-串联质谱法(SPME-portable GC-MS/MS)现场测定水中的2-甲基异莰醇(2-MIB)和土臭素(GSM)的方法。优化了选择反应监测(SRM)的仪器条件,考察了SPME方法的搅拌速度、萃取时间、萃取温度对富集效果的影响,确定最佳的实验条件为:搅拌速度1200 r/min,萃取温度70℃,萃取时间40 min。2-MIB和GSM方法的检出限(LOD)分别为1.1和0.5 ng/L,定量限(LOQ)分别为3.6和1.8 ng/L,线性范围为5～100 ng/L,相关系数分别为0.9922和0.9996。目标物加标浓度为10～100 ng/L时,平均回收率在91.5%～107.9%之间,相对标准偏差(RSD)≤10.1%(n=6)。本方法结合了SPME法操作简单、快捷和串联质谱法高灵敏度、高选择性的优点,现场检测性能可达到实验室标准方法水平,适于水中2-MIB和GSM的现场分析检测。
A solid phase micro-extraction coupled with portable gas chromatography-tandem mass spectrometry method for field analysis was developed for the determination of 2-methylisoborneol(2-MIB)and geosmin(GSM)in water. The selective reaction monitoring(SRM)parameters were optimized. The SPME conditions such as stirring rate, extraction time and extraction temperature were investigated. Optimum SPME conditions were as follows: stirring rate of 1200 r/min, extraction time of 40 min, extraction temperature of 70℃. Limits of detection of 2-MIB and GSM were 1.1 ng/L and 0.5 ng/L respectively. Limits of quantification were 3.6 ng/L and 1.8 ng/L respectively. Linear detection range was 5-100 ng/L with correlation coefficients of 0.9922 and 0.9996, respectively. At the spiked level of 10-100 ng/L, the average recoveries of target compounds were 91.5%-107.9% with RSDs≤10.1%(n=6). This method combines simplicity and rapidtity of SPME and high sensitivity and high selectivity of tandem mass spectrometry, and performance of the method is comparable to that of national standard method. It is especially suitable for the field determination of 2-MIB and geosmin GSM in real water samples.
A solid phase micro-extraction coupled with portable gas chromatography-tandem mass spectrometry method for field analysis was developed for the determination of 2-methylisoborneol(2-MIB)and geosmin(GSM)in water. The selective reaction monitoring(SRM)parameters were optimized. The SPME conditions such as stirring rate, extraction time and extraction temperature were investigated. Optimum SPME conditions were as follows: stirring rate of 1200 r/min, extraction time of 40 min, extraction temperature of 70℃. Limits of detection of 2-MIB and GSM were 1.1 ng/L and 0.5 ng/L respectively. Limits of quantification were 3.6 ng/L and 1.8 ng/L respectively. Linear detection range was 5-100 ng/L with correlation coefficients of 0.9922 and 0.9996, respectively. At the spiked level of 10-100 ng/L, the average recoveries of target compounds were 91.5%-107.9% with RSDs≤10.1%(n=6). This method combines simplicity and rapidtity of SPME and high sensitivity and high selectivity of tandem mass spectrometry, and performance of the method is comparable to that of national standard method. It is especially suitable for the field determination of 2-MIB and geosmin GSM in real water samples.
引文
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2 Medsker L L, Jenkins D, Thomas J F, Koch C. Environ. Sci. Technol., 1969, 3(5): 476-477
3 Watson S B. Phycologia, 2003, 42(4): 333-350
4 Benanou D, Acobas F, De Roubin M R, David F, Sandra P. Anal. Bioanal. Chem., 2003, 376(1): 69-77
5 GB 5749-2006, Standards for Drinking Water Quality. National Standards of the People's Republic of China饮用水卫生标准. 中华人民共和国国家标准. GB 5749-2006
6 XU Ying, LI Wen, WU Wen-Zhong, ZHANG Yong-Yuan. Acta Ecologica Sinica, 1999, 19(2): 212-216 徐盈, 黎雯, 吴文忠, 张甬元. 生态学报, 1999, 19(2): 212-216
7 MA Xiao-Yan, GAO Nai-Yun, LI Qing-Song, LIU Cheng, GU Guo-Fen. Environmental Science, 2008, 29(4): 902-908 马晓雁, 高乃云, 李青松, 刘成, 顾国芬. 环境科学, 2008, 29(4): 902-908
8 Shin H S, Ahn H S. Chromatographia, 2004, 59(1): 107-119
9 MA Lan, ZENG Ning, SUN Xin, LIU Ling-Wei. Chinese Journal of Environmental Engineering, 2017, 11(5): 3304-3311马兰, 曾宁, 孙昕, 刘凌炜. 环境工程学报, 2017, 11(5): 3304-3311
10 ZHU Shuai, JIA Jing, RAO Zhu, LU Guo-Hui, SHEN Ya-Ting. Environmental Chemistry, 2016, 35(10): 2127-2133朱帅, 贾静, 饶竹, 路国慧, 沈亚婷. 环境化学, 2016, 35(10): 2127-2133
11 Nakamura S, NakaInura N, Ito S. J. Sep. Sci., 2001, 24(8): 674-677
12 MAO Min-Min, ZHANG Ke-Jia, ZHANG Tu-Qiao, LI Cong. Chinese J. Anal. Chem., 2013, 41(5): 760-765 毛敏敏, 张可佳, 张土乔, 李聪. 分析化学, 2013, 41(5): 760-765
13 Ma K, Zhang J N, Zhao M, He Y J. J. Sep. Sci., 2012, 35(12): 1494-1501
14 CHENG Jian-Guo, LIU Kai-Ying, BAI Min-Dong, CHENG Chao, YU Yi-Xuan, ZHOU Xin-Ying. Chinese Journal of Chromatography, 2015, 33(12): 1287-1293成建国, 刘开颖, 白敏冬, 程超, 余忆玄, 周新颖. 色谱, 2015, 33(12): 1287-1293
15 Machado S, Gonc?alves C, Cunha E, Guimaraes A, Alpendurada M F. Talanta, 2011, 84(4): 1133-1140
16 GB/T 32470-2016, Organic Compounds in Drinking Water-Test method of Geosmin and 2-Methylisoborneol. National Standards of the People's Republic of China生活饮用水臭味物质土臭素和2-甲基异莰醇检验方法. 中华人民共和国国家标准. GB/T 32470-2016
17 YU Xuan-Yi, CHEN Feng, HUA Bo. Environmental Science and Technology, 2015, 28(1): 48-53誉绚仪, 陈锋, 华勃. 环境科技, 2015, 28(1): 48-53
18 Barreira L M F, Parshintsev J, K?rkk?inen N, Hartonen K, Jussila M, Kajos M, Kulmala M, Riekkola M L. Atmos. Environ., 2015, 115: 214-222
19 Zhao Y, Liu M Y. Procedia Eng., 2014, 84: 731-735
20 Grandy J J, Boyaci E, Pawliszyn J. Anal. Chem., 2016, 88(3): 1760-1767
2 Medsker L L, Jenkins D, Thomas J F, Koch C. Environ. Sci. Technol., 1969, 3(5): 476-477
3 Watson S B. Phycologia, 2003, 42(4): 333-350
4 Benanou D, Acobas F, De Roubin M R, David F, Sandra P. Anal. Bioanal. Chem., 2003, 376(1): 69-77
5 GB 5749-2006, Standards for Drinking Water Quality. National Standards of the People's Republic of China饮用水卫生标准. 中华人民共和国国家标准. GB 5749-2006
6 XU Ying, LI Wen, WU Wen-Zhong, ZHANG Yong-Yuan. Acta Ecologica Sinica, 1999, 19(2): 212-216 徐盈, 黎雯, 吴文忠, 张甬元. 生态学报, 1999, 19(2): 212-216
7 MA Xiao-Yan, GAO Nai-Yun, LI Qing-Song, LIU Cheng, GU Guo-Fen. Environmental Science, 2008, 29(4): 902-908 马晓雁, 高乃云, 李青松, 刘成, 顾国芬. 环境科学, 2008, 29(4): 902-908
8 Shin H S, Ahn H S. Chromatographia, 2004, 59(1): 107-119
9 MA Lan, ZENG Ning, SUN Xin, LIU Ling-Wei. Chinese Journal of Environmental Engineering, 2017, 11(5): 3304-3311马兰, 曾宁, 孙昕, 刘凌炜. 环境工程学报, 2017, 11(5): 3304-3311
10 ZHU Shuai, JIA Jing, RAO Zhu, LU Guo-Hui, SHEN Ya-Ting. Environmental Chemistry, 2016, 35(10): 2127-2133朱帅, 贾静, 饶竹, 路国慧, 沈亚婷. 环境化学, 2016, 35(10): 2127-2133
11 Nakamura S, NakaInura N, Ito S. J. Sep. Sci., 2001, 24(8): 674-677
12 MAO Min-Min, ZHANG Ke-Jia, ZHANG Tu-Qiao, LI Cong. Chinese J. Anal. Chem., 2013, 41(5): 760-765 毛敏敏, 张可佳, 张土乔, 李聪. 分析化学, 2013, 41(5): 760-765
13 Ma K, Zhang J N, Zhao M, He Y J. J. Sep. Sci., 2012, 35(12): 1494-1501
14 CHENG Jian-Guo, LIU Kai-Ying, BAI Min-Dong, CHENG Chao, YU Yi-Xuan, ZHOU Xin-Ying. Chinese Journal of Chromatography, 2015, 33(12): 1287-1293成建国, 刘开颖, 白敏冬, 程超, 余忆玄, 周新颖. 色谱, 2015, 33(12): 1287-1293
15 Machado S, Gonc?alves C, Cunha E, Guimaraes A, Alpendurada M F. Talanta, 2011, 84(4): 1133-1140
16 GB/T 32470-2016, Organic Compounds in Drinking Water-Test method of Geosmin and 2-Methylisoborneol. National Standards of the People's Republic of China生活饮用水臭味物质土臭素和2-甲基异莰醇检验方法. 中华人民共和国国家标准. GB/T 32470-2016
17 YU Xuan-Yi, CHEN Feng, HUA Bo. Environmental Science and Technology, 2015, 28(1): 48-53誉绚仪, 陈锋, 华勃. 环境科技, 2015, 28(1): 48-53
18 Barreira L M F, Parshintsev J, K?rkk?inen N, Hartonen K, Jussila M, Kajos M, Kulmala M, Riekkola M L. Atmos. Environ., 2015, 115: 214-222
19 Zhao Y, Liu M Y. Procedia Eng., 2014, 84: 731-735
20 Grandy J J, Boyaci E, Pawliszyn J. Anal. Chem., 2016, 88(3): 1760-1767